CN102839394B - Method for rapidly preparing tree-like nano-iron with multi-level structure - Google Patents
Method for rapidly preparing tree-like nano-iron with multi-level structure Download PDFInfo
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- CN102839394B CN102839394B CN201210344112.XA CN201210344112A CN102839394B CN 102839394 B CN102839394 B CN 102839394B CN 201210344112 A CN201210344112 A CN 201210344112A CN 102839394 B CN102839394 B CN 102839394B
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Abstract
The invention discloses a method for rapidly preparing tree-like nano-iron with a multi-level structure, which relates to a method for preparing tree-like nano-iron and is used for solving the problems of incapability of directly preparing tree-like nano-iron with the multi-level structure and low purity, long period, toxicity, pollution and high cost of the prepared tree-like nano-iron with the multi-level structure in the prior art. The method comprises the following steps of: I, selecting a selectively-permeable membrane reactor; II, preparing a cathode electrolyte and an anode electrolyte; III, injecting the electrolytes into a reactive tank; IV, reacting; and V, collecting, washing and drying. Due to the adoption of the method, tree-like nano-iron with the multi-level structure can be prepared directly; according to an XRD (X-Ray Diffraction) spectrogram of a product, the tree-like nano-iron with the multi-level structure prepared with the method is free from remarkable impurity peaks, is free from impurity peaks at small angles, and has high purity; the preparation speed of the tree-like nano-iron is high, and the period is short; a toxic and harmful potassium ferricyanide raw material is not used, and cost is lowered. The method is used for preparing tree-like nano-iron with the multi-level structure.
Description
Technical field
The present invention relates to a kind of method of preparing dendritic Nanoscale Iron.
Background technology
In some fields, as ore dressing, (main component is Fe in the Industrial processes such as printing and dyeing and plating, can to produce a large amount of waste water containing iron ion
2+and Fe
3+), if not treated being directly discharged in environment of these waste water not only has serious harm to environment, but also waste a large amount of resources.Meanwhile, nano-level iron, the dendritic iron especially with micro nano structure has very high Application Areas and economic value added, just has very large practical significance as how lower cost obtains dendritic micro-nano iron powder fast.The object of this experiment is exactly the iron powder that makes micro nano structure by the lower ferrous sulfate of electrochemical method reduction price, and utilize the method to reclaim the iron in iron rust and rich iron ion waste water, produce the multistage dendritic nanometer iron powder of higher degree, make the iron in these iron rust and rich iron ion waste water become the multistage dendritic nanometer iron powder with high economic value added, turn waste into wealth, this also can embody the idea of development of our national resources recycle and Sustainable development simultaneously.
Nano material, due to its unique physicochemical property, has extremely important researching value and application prospect in the every field such as scientific research and social production.Be emphasis and the focus of research both at home and abroad to the research of nano material, wherein the synthetic preparation of nano material is again the most important thing always.The nano material of iron has a wide range of applications in the field such as catalysis and microelectronics, therefore also becomes the focus of research instantly.The dendritic Nanoscale Iron of multilevel hierarchy is mainly used in suction ripple, and the high-tech areas such as electromagnetism and catalysis are different from traditional electrolytic iron, have very high economic value added.
At present very extensive to the research of dendritic nano material, in document, report that many materials all have this structure, as metal, metallic sulfide and metal oxide etc., preparing now dendritic nano material is mainly to adopt hydro-thermal or solvent-thermal method, ultrasonic wave auxiliary law and metal replacement reduction method.According to existing bibliographical information, hydro-thermal, solvent thermal and ultrasonic wave auxiliary law production cycle are long, cannot directly prepare the dendritic nano material of metal, and use the poisonous and hazardous Tripotassium iron hexacyanide (K
3[Fe (CN)
6]) starting material, cost is high; Metal replacement method, cannot direct replacement tap a blast furnace, and throughput rate is slow.These factors have greatly limited the quick production of the dendritic Nanoscale Iron of multilevel hierarchy.There is researchist once to make dendritic Nanoscale Iron, but be by first preparing dendritic Fe
2o
3, then utilize hydrogen reducing, make the dendritic Nanoscale Iron of multilevel hierarchy.And directly do not make the Nanoscale Iron of multilevel hierarchy.
Therefore, exist prior art cannot directly make the dendritic Nanoscale Iron of multilevel hierarchy, the dendritic Nanoscale Iron purity of the multilevel hierarchy of making is low, and the cycle is long, poisonous have pollute and the high problem of cost.
Summary of the invention
The present invention is the dendritic Nanoscale Iron that will solve prior art and cannot directly make multilevel hierarchy, the dendritic Nanoscale Iron purity of the multilevel hierarchy of making is low, cycle is long, and poisonous have pollution and the high problem of cost, and a kind of method of the dendritic Nanoscale Iron of preparing fast multilevel hierarchy is provided.
Prepare fast a method for the dendritic Nanoscale Iron of multilevel hierarchy, specifically prepare according to following steps:
One, get 1 cover permselectivity membrane reactor; Wherein, this permselectivity membrane reactor is made up of reactive tank (2), permselectivity membrane (3), negative electrode (4), anode (5) and the wire (6) of direct supply (1), band cooling jacket (7); In the reactive tank (2) of band cooling jacket (7), permselectivity membrane (3) is set reactive tank (2) is divided into positive column and cathodic area, the positive pole of direct supply (1) is connected with anode (5) by wire (6) and anode (5) is put into reactive tank (2) positive column, and the negative pole of direct supply (1) is connected with negative electrode (4) by wire (6) and negative electrode (4) is put into reactive tank (2) cathodic area; Permselectivity membrane (3) is negatively charged ion perviousness film, allows negatively charged ion pass through, and positively charged ion does not pass through; Cooling jacket (7) arranges water-in (7-1) and water outlet (7-2);
Two, be that 100g/L～400g/L, ethanol content are 50ml/L～60ml/L by iron concentration, take molysite and ethanol and join in deionized water, mix, obtain catholyte; Be 0.1mol/L～1mol/L by sulfuric acid concentration, preparation dilute sulphuric acid, obtains anolyte;
Three, pass into the water of 15 DEG C～25 DEG C and derive from water outlet (7-2) to the water-in (7-1) of cooling jacket (7), catholyte is injected in cathodic area to reactive tank (2), injects anolyte to the positive column of reactive tank (2); Wherein, the volume ratio of catholyte and anolyte is 3～1:1;
Four, the direct supply (1) of opening permselectivity membrane reactor, the surface current density of control cathode (4) is 10A/cm
2～20A/cm
2; Every 1min～3min stopped reaction in reaction process, takes out negative electrode (4) and collects after product, then negative electrode (4) is put into reactive tank (2) and proceed;
Five, the product of collection is put into sealed vessel, by washed with de-ionized water, wash with alcohol, then put into vacuum drying oven again, controlling temperature is 50 DEG C～60 DEG C, and insulation 3h～4h obtains the dendritic Nanoscale Iron of multilevel hierarchy.
The dendritic Nanoscale Iron of multilevel hierarchy prepared by the present invention is filled with inert gas seal and preserves.
Reaction principle of the present invention:
In real reaction process, in ferrous sulfate electrolytic solution mainly there are following two reactions in the negative electrode of (concentration of electrolyte is 250g/L):
Fe
2++2e
-＝Fe (1)
2H
++2e
-＝H
2 (2)
In the starting stage of reaction, the speed of negative electrode generation iron simple substance is very fast, and only has a small amount of gas (H
2) separate out, main reaction (1) is reduced to iron for ferrous ion.Calculate in theory to confirm from electrochemical electrode electromotive force:
The equilibrium potential of reaction (1): E
(Fe2+|Fe)=E
0 (Fe2+, Fe)-RT/2F (lna
fe2+ -1) (3)
(the equilibrium potential E under its normal conditions
0 (Fe2+, Fe)=-0.44V)
The equilibrium potential of reaction (2): E
(2H+|H2)=E
0 (2H+|H2)-RT/2F (lna
h+ -1) (4)
(the equilibrium potential E under its normal conditions
0 (2H+|H2)=0V)
E under the normal conditions
0 (2H+|H2)>E
0 (Fe2+, Fe), therefore hydrogen will be separated out prior to iron.Known according to (4) formula, in solution, hydrogen ion concentration is higher, E
(2H+|H2)larger, thereby be more conducive to separating out of hydrogen.So hydrogen ion concentration is less, PH is higher, is conducive to E
(2H+|H2)reduce, just can make E
(Fe2+, Fe)there is the E of being greater than
(2H+|H2)possibility, separate out iron simple substance.Also proved above-mentioned rule through overtesting.Now reaction is main generates iron simple substance, and speed of reaction is fast.
All the time mainly there is oxygen evolution reaction for anode and generate hydrogen ion simultaneously:
H
2O-2e
-＝2H
++1/2O
2 (5)
But after reaction proceeds to certain hour, the hydrogen ion that electrolytic solution Anodic discharges runs up to finite concentration reduces the pH value of electrolytic solution, can affect the reduction reaction of negative electrode.Make the decomposition voltage (E of hydrogen ion decomposition voltage higher than ferrous ion
0 (2H+|H2)>E
0 (Fe2+, Fe)), so cathodic reaction taking evolving hydrogen reaction (2) as main, and the generating rate of iron simple substance is die-offed, electrolyte temperature raises fast simultaneously, power-efficient reduces.The electrochemical electrode electromotive force of reaction (5) is expressed as:
E
0(O
2|H
2O)＝+1.229V (6)
Therefore need to make hydrogen ion cannot be diffused into negative electrode with negatively charged ion permselectivity membrane, keep negative electrode always taking reflection (1) as main reaction.
The invention has the beneficial effects as follows: the present invention can directly prepare the dendritic Nanoscale Iron of multilevel hierarchy; Can find out that from the XRD spectra of product dendritic Nanoscale Iron that the present invention prepares multilevel hierarchy is without obvious impurity peaks, and Small angle inclusion-free peak, therefore the purity of product is higher; The speed of the dendritic Nanoscale Iron that the present invention obtains is 0.05g～0.1g/min, and throughput rate is fast, and the cycle is short; The present invention does not use the poisonous and hazardous Tripotassium iron hexacyanide (K
3[Fe (CN)
6]) starting material, and reduced cost.
The present invention is for the preparation of dendritic Nanoscale Iron.
Brief description of the drawings
Fig. 1 is the device schematic diagram of the selection perviousness film reactor that uses of the present invention, wherein 1 for direct supply, 2 for reactive tank, 3 for permselectivity membrane, 4 for negative electrode, 5 for anode, 6 for wire, 7 for cooling jacket, 7-1 be that water-in, 7-2 are water outlet.
Fig. 2 is 25000 times of scanning electron microscope (SEM) photographs of the dendritic Nanoscale Iron of the multilevel hierarchy prepared of embodiment mono-.
Fig. 3 is 10000 times of scanning electron microscope (SEM) photographs of the dendritic Nanoscale Iron of the multilevel hierarchy prepared of embodiment mono-.
Fig. 4 is the XRD spectra of the dendritic Nanoscale Iron of the multilevel hierarchy prepared of embodiment mono-, and wherein " ■ " represents the diffraction peak of Fe.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method for a kind of dendritic Nanoscale Iron of preparing fast multilevel hierarchy of present embodiment, specifically prepare according to following steps:
One, get 1 cover permselectivity membrane reactor; Wherein, this permselectivity membrane reactor (referring to accompanying drawing 1) is made up of direct supply 1, reactive tank 2, permselectivity membrane 3, negative electrode 4, anode 5 and wire 6 with cooling jacket 7; In reactive tank 2 with cooling jacket 7, permselectivity membrane 3 is set reactive tank 2 is divided into positive column and cathodic area, the positive pole of direct supply 1 is connected with anode 5 by wire 6 and anode 5 is put into reactive tank 2 positive columns, and the negative pole of direct supply 1 is connected with negative electrode 4 by wire 6 and negative electrode 4 is put into reactive tank 2 cathodic areas; Permselectivity membrane 3 is negatively charged ion perviousness films, allows negatively charged ion pass through, and positively charged ion does not pass through; Cooling jacket 7 arranges water-in 7-1 and water outlet 7-2;
Two, be that 100g/L～400g/L, ethanol content are 50ml/L～60ml/L by iron concentration, take molysite and ethanol and join in deionized water, mix, obtain catholyte; Be 0.1mol/L～1mol/L by sulfuric acid concentration, preparation dilute sulphuric acid, obtains anolyte;
Three, pass into the water of 15 DEG C～25 DEG C and derive from water outlet 7-2 to the water-in 7-1 of cooling jacket 7, injecting catholyte to the cathodic area of reactive tank 2, injecting anolyte to the positive column of reactive tank 2; Wherein, the volume ratio of catholyte and anolyte is 3～1:1;
Four, open the direct supply 1 of permselectivity membrane reactor, the surface current density of control cathode 4 is 10A/cm
2～20A/cm
2; Every 1min～3min stopped reaction in reaction process, takes out negative electrode 4 and collects after product, then negative electrode 4 is put into reactive tank 2 and proceed;
Five, the product of collection is put into sealed vessel, by washed with de-ionized water, wash with alcohol, then put into vacuum drying oven again, controlling temperature is 50 DEG C～60 DEG C, and insulation 3h～4h obtains the dendritic Nanoscale Iron of multilevel hierarchy.
The dendritic Nanoscale Iron of multilevel hierarchy prepared by present embodiment is filled with inert gas seal and preserves.
Embodiment two: present embodiment is different from embodiment one: in step 1, negative electrode 4 is that copper electrode, anode 5 are graphite cake.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: in step 2, in catholyte, iron concentration is that 200g/L～300g/L, ethanol content are 52ml/L～58ml/L, and in anolyte, sulfuric acid concentration is 0.2mol/L～0.9mol/L.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: in step 2, molysite is ferrous sulfate or iron protochloride.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: in step 4, the surface current density of negative electrode 4 is 12A/cm
2～18A/cm
2.Other is identical with one of embodiment one to four.
The definition of surface current density: surface current density=electric current/electrode surface area
Adopt following examples and contrast experiment to verify beneficial effect of the present invention:
Embodiment mono-:
The method of a kind of dendritic Nanoscale Iron of preparing fast multilevel hierarchy of the present embodiment, specifically prepare according to following steps:
One, get 1 cover permselectivity membrane reactor; Wherein negative electrode 4 is copper electrode, and anode 5 is graphite cake, and permselectivity membrane 3 is negatively charged ion perviousness films;
Two, be that 200g/L, ethanol content are 50mL/L by iron concentration, take ferrous sulfate and ethanol and join in deionized water, mix, obtain catholyte; Be 0.5mol/L by sulfuric acid concentration, preparation dilute sulphuric acid, obtains anolyte;
Three, pass into the water of 20 DEG C and derive from water outlet 7-2 to the water-in 7-1 of cooling jacket 7, injecting 200mL catholyte to the cathodic area of reactive tank 2, injecting 200mL anolyte to the positive column of reactive tank 2;
Four, open the direct supply 1 of permselectivity membrane reactor, the surface current density of control cathode 4 is 15A/cm
2; Every 3min stopped reaction in reaction process, takes out negative electrode 4 and collects after product, then negative electrode 4 is put into reactive tank 2 and proceed;
Five, the product of collection is put into sealed vessel, by the washed with de-ionized water 3 times of boiling, wash 3 times with alcohol, then put into vacuum drying oven again, controlling temperature is 50 DEG C, and insulation 3h obtains the dendritic Nanoscale Iron of multilevel hierarchy.
The dendritic Nanoscale Iron of multilevel hierarchy prepared by the present embodiment is filled with nitrogen-sealed and preserves.
The scanning electron microscope (SEM) photograph of the dendritic Nanoscale Iron of multilevel hierarchy prepared by the present embodiment is as shown in Fig. 2 Fig. 3, as can be seen from the figure the dendritic Nanoscale Iron that the product that prepared by the present invention is multilevel hierarchy, its width, at 2 microns, is released souls from purgatory at 8 microns, the similar branch of shape, and there is face and branch anyway.
As shown in Figure 4, wherein " ■ " represents the diffraction peak of Fe to the XRD spectra of the dendritic Nanoscale Iron of multilevel hierarchy prepared by the present embodiment; As can be seen from the figure its structure is body-centered cubic structure, obviously impurity peaks of nothing in figure, and Small angle inclusion-free peak, and therefore the purity of product is higher.
The speed of the dendritic Nanoscale Iron of multilevel hierarchy prepared by the present embodiment is 0.08g/min, and throughput rate is fast.
Claims (5)
1. prepare fast a method for the dendritic Nanoscale Iron of multilevel hierarchy, it is characterized in that the method for the dendritic Nanoscale Iron of preparing fast multilevel hierarchy, specifically prepare according to following steps:
One, get 1 cover permselectivity membrane reactor; Wherein, this permselectivity membrane reactor is made up of reactive tank (2), permselectivity membrane (3), negative electrode (4), anode (5) and the wire (6) of direct supply (1), band cooling jacket (7); In the reactive tank (2) of band cooling jacket (7), permselectivity membrane (3) is set reactive tank (2) is divided into positive column and cathodic area, the positive pole of direct supply (1) is connected with anode (5) by wire (6) and anode (5) is put into reactive tank (2) positive column, and the negative pole of direct supply (1) is connected with negative electrode (4) by wire (6) and negative electrode (4) is put into reactive tank (2) cathodic area; Permselectivity membrane (3) is negatively charged ion perviousness film; Cooling jacket (7) arranges water-in (7-1) and water outlet (7-2);
Two, be that 100g/L ~ 400g/L, ethanol content are 50ml/L ~ 60ml/L by iron concentration, take molysite and ethanol and join in deionized water, mix, obtain catholyte; Be 0.1mol/L ~ 1mol/L by sulfuric acid concentration, preparation dilute sulphuric acid, obtains anolyte;
Three, pass into the water of 15 DEG C ~ 25 DEG C and derive from water outlet (7-2) to the water-in (7-1) of cooling jacket (7), catholyte is injected in cathodic area to reactive tank (2), injects anolyte to the positive column of reactive tank (2); Wherein, the volume ratio of catholyte and anolyte is 3 ~ 1:1;
Four, the direct supply (1) of opening permselectivity membrane reactor, the surface current density of control cathode (4) is 10A/cm
2~ 20A/cm
2; Every 1min ~ 3min stopped reaction in reaction process, takes out negative electrode (4) and collects after product, then negative electrode (4) is put into reactive tank (2) and proceed;
Five, the product of collection is put into sealed vessel, by washed with de-ionized water, wash with alcohol, then put into vacuum drying oven again, controlling temperature is 50 DEG C ~ 60 DEG C, and insulation 3h ~ 4h obtains the dendritic Nanoscale Iron of multilevel hierarchy.
2. the method for a kind of dendritic Nanoscale Iron of preparing fast multilevel hierarchy according to claim 1, is characterized in that negative electrode in step 1 (4) is that copper electrode, anode (5) are graphite cake.
3. the method for a kind of dendritic Nanoscale Iron of preparing fast multilevel hierarchy according to claim 2, it is characterized in that in step 2 in catholyte that iron concentration is that 200g/L ~ 300g/L, ethanol content are 52ml/L ~ 58ml/L, in anolyte, sulfuric acid concentration is 0.2mol/L ~ 0.9mol/L.
4. the method for a kind of dendritic Nanoscale Iron of preparing fast multilevel hierarchy according to claim 3, is characterized in that in step 2, molysite is ferrous sulfate or iron protochloride.
5. the method for a kind of dendritic Nanoscale Iron of preparing fast multilevel hierarchy according to claim 4, the surface current density that it is characterized in that negative electrode in step 4 (4) is 12A/cm
2~ 18A/cm
2.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104928725B (en) * | 2015-07-07 | 2017-07-28 | 哈尔滨工业大学 | A kind of method for efficiently preparing dendritic α Fe absorbing materials |
| CN105018971B (en) * | 2015-07-20 | 2017-09-12 | 哈尔滨工业大学 | A kind of method by the dendritic α Fe sills of iron standby functional micro-nano structure |
| CN107008326B (en) * | 2017-05-15 | 2019-04-16 | 哈尔滨工业大学 | A kind of preparation method of the carbon quantum dot load efficient out-phase class fenton catalyst of iron-based material |
| CN109616330B (en) * | 2018-10-31 | 2021-06-01 | 中山大学 | Metal oxide/metal composite nano dendritic structure material and preparation method thereof |
| CN115403195B (en) * | 2022-08-23 | 2024-03-29 | 哈尔滨工业大学 | Method for treating organic wastewater by utilizing micro-nano dendritic zero-valent copper catalyst to activate molecular oxygen |
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